Laboratório de Ressonância Magnética Nuclear-Departamento de Química, Universidade Federal de São Carlos, Rod. Washington Luís, Km 235, C.P. 676, CEP 13565-905, São Carlos, SP, Brazil.
Analyst. 2012 May 21;137(10):2357-61. doi: 10.1039/c2an16208c. Epub 2012 Mar 28.
Hyphenated HPLC-NMR is an extremely efficient analytical tool, which makes it possible to perform on-flow experiments where 1D NMR spectra are obtained in real time as the analytes are separated and eluted from the chromatographic column. However, it is incompatible with multidimensional NMR methods that form an indispensible tool for the study of complex mixtures. Recently, Frydman and co-workers have proposed an ultrafast 2D NMR approach, where a complete 2D NMR correlation can be recorded in a single scan, thus providing a solution to the irreversibility of hyphenated techniques. This paper presents the first implementation of on-line ultrafast HPLC-NMR. Ultrafast COSY spectra are acquired every 12 s in the course of a chromatographic run performed on a mixture of natural aromatic compounds. The results, obtained on a commercial HPLC-NMR setup, highlight the generality of the ultrafast HPLC-NMR methodology, thus opening the way to a number of applications in the numerous fields in which HPLC-NMR forms a routine analytical tool.
带连线的 HPLC-NMR 是一种非常高效的分析工具，它可以实现在线实验，在色谱柱分离和洗脱分析物的同时实时获得 1D NMR 谱。然而，它与多维 NMR 方法不兼容，多维 NMR 方法是研究复杂混合物不可或缺的工具。最近，Frydman 及其同事提出了一种超快 2D NMR 方法，其中可以在单个扫描中记录完整的 2D NMR 相关谱，从而为解决连线技术的不可逆性提供了一种解决方案。本文介绍了在线超快 HPLC-NMR 的首次实现。在对天然芳香族化合物混合物进行的色谱运行过程中，每 12 s 采集一次超快 COSY 谱。在商业 HPLC-NMR 装置上获得的结果突出了超快 HPLC-NMR 方法的通用性，从而为 HPLC-NMR 作为常规分析工具的众多领域中的许多应用开辟了道路。
